An automated SPS-GC-TCD has been optimized to determine hydrogen production in light driven synthesis reactions while operating in real time and being capable of multiple analysis per hour. The SPS-GC-TCD method incorporates two sample loops on a valve, one for a check standard and the other for the sample, eliminating many sources of error associated with gas sampling and allowing for automated calibration during each analytical run. Gas samples containing hydrogen in a percent volume concentration were analyzed and method detection limit (MDL), accuracy and precision measurments have been conducted. Using single point standardization, proof of concept results for the analyzer gave an MDL of 0.73% (v/v%), accuracy of 100%, and precision of 3.7% for hydrogen. These values were comparable to results obtained by a much more intensive 5-point external calibration. The automated system gave extreme improvements in reproducibility, and a detection limit of 0.25% and precision of 1.7%
